La3Cu4P4O2 and La5Cu4P4O4Cl2: synthesis, structure and 31P solid state NMR spectroscopy
Zeitschrift für Naturforschung B(2015)
Abstract
Abstract The phosphide oxides La3Cu4P4O2 and La5Cu4 P4O4Cl2 were synthesized from lanthanum, copper(I) oxide, red phosphorus, and lanthanum(III) chloride through a ceramic technique. Single crystals can be grown in a NaCl/KCl flux. Both structures were refined from single crystal X-ray diffractometer data: I4/mmm, a = 403.89(4), c = 2681.7(3) pm, wR2 = 0.0660, 269 F2 values, 19 variables for La3Cu4P4O2 and a = 407.52(5), c = 4056.8(7) pm, wR2 = 0.0905, 426 F2 values, 27 variables for La5Cu4P4O4Cl2. Refinement of the occupancy parameters revealed full occupancy for the oxygen sites in both compounds. The structures are composed of cationic (La2O2)2+ layers and covalently bonded (Cu4P4)5– polyanionic layers with metallic characteristics, and an additional La3+ between two adjacent (Cu4P4)5– layers. The structure of La5Cu4P4O4Cl2 comprises two additional LaOCl slabs per unit cell. Temperature-dependent magnetic susceptibility studies revealed Pauli paramagnetism. The phosphide substructure of La3Cu4P4O2 was studied by 31P solid state NMR spectroscopy. By using a suitable dipolar re-coupling approach the two distinct resonances belonging to the P2 4– and the P3– units could be identified.
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